Patent GB-531621-A (GB)
Title: Improvements in or relating to sulphonation
IPC: C09K23/00
Filed: 1939-07-06
Abstract: 531,621. Wetting 8 c. agents. COLGATEPALMOLIVE-PEET Co. July 6, 1939, No.. 19668. Convention date, July 7, 1938. [Classes 2 (iii) and 15 (ii)] [Also in Groups III and VI] A coal tar distillate is subjected to sulphonation while dissolved in liquid sulphur dioxide. Tars obtained by the hydrogenation. destructive distillation or liquefication of coal, lignite or peat and coke oven and low temperatures tars may be used as starting material. In examples, fractions distilled from tar produced by low temperature carbonization of West Pennsylvania bituminous coal are employed. The distillate is purified with caustic alkali and 5 per cent. sulphuric acid and re-distilled before being dissolved in liquid sulphur dioxide and sulphonated with oleum or chlorsulphonic acid. The product is worked up by diluting, distilling off the sulphur dioxide, washing out the unattacked hydrocarbons by means of gasoline or ether, boiling with caustic soda lye and drying. The sulphonation is effected with cooling below 0C. in an autoclave. Dichlorethylene, ethylenedichloride, propylenedichloride, dichlorether, monochlorbenzene and carbontetrachloride may be used for extracting unsulphonated material. Sodium chlorsulphonate is mentioned as a sulphonating agent. Unreacted hydrocarbons may also be separated by maintaining the reaction mixture under pressure while adding water to cause the separation of a layer of liquid sulphur dioxide, which contains most of the unreacted material. The product may be freed from inorganic sulphates by extraction with isopropyl, butyl or other alcohol or by forming the calcium salt and separating the calcium sulphate. Ammonium, sodium, magnesium, potassium, triethanolamine and other salts may be prepared by double decomposition using ammonium carbonate, oxalate or phosphate. The sulphonation process may be continuous. The products, which are stated to be wetting, emulsifying, washing and foaming agents may be used alone or with sodium carbonate, resinates, sulphonated compounds, dyes, lakes, pigments, sodium borate, fillers, softeners, perfumes, abrasives, phenols, mercury chloride, phenylmercury nitrate, carbon-tetrachloride, soaps, fats, oils, waxes, glycerine, triethanolamine, pine oil, naphtha, sodium hypochlorite, phosphates, diethyleneglycol, pumice, bentonite and sodium thiosulphate. They may be used in the manufacture of disperions of mineral and vegetable oils, paraffin, asphalt, tar, bitumen, sulphur, rubber, resins, hydrocarbons and higher alcohols and they may be incorporated in cosmetics, shaving creams, dental creams, shampoos, paints, varnishes, lacquers, wood preservatives, solid oils, mayonnaise, ice cream, rootbeer, margarine, agricultural sprays, laxatives, papercoatings. polishes, inks, moulddressings, confections, dye emulsions, photographic emulsions, medicinal and pharmaceutical emulsions and cutting and lubricating oils. They are useful in the flotation of ores, treating textiles and facilitating chemical reactions by emulsifying the reaction liquids, e.g. alkylhalides and aqueous ammonia. Preparations for use on the skin may be prepared by mixing the products with vitamins or compounds capable of forming vitamins. Thus sterols may be subjected to ultraviolet, infrared, radioactive or Rontgen rays and then mixed with the products.